SIST EN ISO 9455-6:2001

SLOVENSKI STANDARD
SIST EN ISO 9455-6:2001
01-februar-2001
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Soft soldering fluxes - Test methods - Part 6: Determination and detection of halide
(excluding fluoride) content (ISO 9455-6:1995)
Flußmittel zum Weichlöten - Prüfverfahren - Teil 6: Bestimmung und Nachweis des
Halogenidgehaltes (außer Fluorid) (ISO 9455-6:1995)
Flux de brasage tendre - Méthodes d'essai - Partie 6: Dosage et détection des
halogénures (a l'exception des fluorures) (ISO 9455-6:1995)
Ta slovenski standard je istoveten z: EN ISO 9455-6:1997
ICS:
25.160.50 Trdo in mehko lotanje Brazing and soldering
SIST EN ISO 9455-6:2001 en
2003-01.Slovenski inštitut za standardizacijo. Razmnoževanje celote ali delov tega standarda ni dovoljeno.

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SIST EN ISO 9455-6:2001

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SIST EN ISO 9455-6:2001

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SIST EN ISO 9455-6:2001

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SIST EN ISO 9455-6:2001

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SIST EN ISO 9455-6:2001

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SIST EN ISO 9455-6:2001
INTERNATIONAL ISO
STANDARD 9455-6
First edition
1995-09-15
Soft soldering fluxes - Test methods -
Part 6:
Determination and detection of halide
(excluding fluoride) content
Flux de brasage tendre - Methodes d’essai -
Partie 6: Dosage et dk tection des halog&wres (2 i’excep tion des fluorures)
Weference number
ISO 9455-6: 1995(E)

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SIST EN ISO 9455-6:2001
ISO 9455-6: 1995(E)
Foreword
ISO (the International Organization for Standardization) is a worldwide
federation of national Standards bodies (ISO member bodies). The work
of preparing International Standards is normally carried out through ISO
technical committees. Esch member body interested in a subject for
which a technical committee has been established has the right to be
represented on that committee. International organizations, governmental
and non-governmental, in liaison with ISO, also take part in the work. ISO
collaborates closely with the International Electrotechnical Commission
(1 EC) on all matters of electrotechnical standardization.
Draft International Standards adopted by the technical committees are
circulated to the member bodies for voting. Publication as an International
Standard requires approval by at least 75 % of the member bodies casting
a vote.
International Standard ISO 9455-6 was prepared by Technical Committee
lSO/TC 44, Weiding and allied processes, Subcommittee SC 12,
Soldering and brazing ma terials.
ISO 9455 consists of the following Parts, under the general title Soft
soldering fluxes - Test methods:
- Part 1: Determination of non-vola tile matter, gravime tric method
- Part 2: Determination of non-vola tile matter, ebulliometric method
- Part 3: Determination of acid value, poten tiome tric and visual
titra tion me thods
- Part 5: Copper mirror test
- Part 6: Determination and detection of halide (excluding fluoride)
content
- Part 8: Determination of zinc con ten t
- Part 9: Determination of ammonia content
- Part 7 0: Flux efficacy tests, solder spread method
- Part I 1: Solubility of flux residues
0 ISO 1995
All rights reserved. Unless otherwise specified, no part of this publication may be reproduced
or utilized in any form or by any means, electronie or mechanical, including photocopying and
mrcrofilm, without Permission in writing from the publisher.
International Organization for Standardization
Case Postale 56 l CH-l 211 Geneve 20 l Switzerland
Printed in Switzerland
ii

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SIST EN ISO 9455-6:2001
0 ISO ISO 9455=6:1995(E)
- Part 72: Steel tube corrosion test
- Part 13: Determination of flux spattering
- Part 14: Assessment of tackiness of flux residues
- Part 15: Copper corrosion test
- Part 16: Flux efficacy tests, wetting balance method
[Technical Report]
- Part 17: Determination of surface insulation resistance of flux resi-
dues (Comb test)
- Part 18: Electrochemical migration test for flux residues
Annex A forms an integral part of this part of ISO 9455.

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SIST EN ISO 9455-6:2001
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SIST EN ISO 9455-6:2001
INTERNATIONAL STANDARD 0 ISO ISO 9455-6: 1995(E)
Soft soldering fluxes - Test methods -
Part 6:
Determination and detection of halide (excluding fluoride)
content
of this part of ISO 9455. At the time of publication, the
1 Scope
editions indicated were valid. All Standards are subject
to revision, and Parties to agreements based on this
This part of ISO 9455 specifies three quantitative
part of ISO 9455 are encouraged to investigate the
methods for the determination of the ionic halide (ex-
possibility of applying the most recent editions of the
cluding fluoride) content of soldering fluxes. Halides
Standards indicated below. Members of IEC and ISO
are calculated as chlorides. A useful qualitative test
maintain registers of currently valid International
method for the detection of ionic halides is also de-
Standards.
scribed.
Method A is a potentiometric titration method for the
ISO 5725-2: 1994, Accuracy (trueness and precision)
determination of halide (excluding fluoride) content of measurement methods and results - Part 2: Basic
and is applicable to flux classes 1 and 2, defined in method for the determination of repeatability and
ISO 9454-1. This method, which is to be considered reproducibility of a Standard measurement method.
the reference method for these fluxes, is suitable
ISO 9454-1: 1990, Soft soldering fluxes - Classifi-
for halide contents generally within the range
ca tion and requiremen ts - Part 7: Classification,
0,05 % (m/m) to 2 % (m/m) in the non-volatile matter
labelling and packaging.
of the flux.
Method B is a titration method for the determination
ISO 9455-1 :1990, Soft soldering fluxes - Test meth-
of the total halide (excluding fluoride) content of
ods - Part 1: Determination of non-vola tile matter,
water-soluble fluxes. lt is applicable to flux classes
gravimetric method.
2.1.2.A and 3.1 .l .A, as defined in ISO 9454-1.
ISO 9455-2:1993, Soft soldering fluxes - Test meth-
Method C is a titration method for the determination
ods - Part 2: Determination of non-volatile matter,
of the halide (excluding fluoride) content of water-
ebulliometric method.
soluble fluxes containing Phosphates and is applica-
ble to flux class 3.2.1 .A, as defined in ISO 9454-1.
Method D is a qualitative test, using silver chromate 3 Method A: Potentiometric method
test Paper, for the presence of ionic halides. The
(Reference method)
technique may be used for all classes of flux.
3.1 Principle
A prepared, weighed Sample of the flux is dissolved
2 Normative references
in a suitable solvent. The resulting Solution is titrated
with Standard silver nitrate solution, using a silver
The following standards contain provisions which,
through reference in this text, constitute provisions electrode, the mV readings being recorded simul-
1

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SIST EN ISO 9455-6:2001
0 ISO
ISO 9455-6: 1995(E)
taneously. From the graph of volume of titrant 3.3.4 Magnetit or mechanical stirrer, with variable
readings against mV readings, the Point of inflexion is Speed drive, the stirrer bar to be PTFE-coated.
determined and the percentage halide content, ex-
pressed as chloride, is calculated. The method is not
3.4 Procedure
suitable for the determination of fluoride.
Carry out the following procedure, in triplicate, on the
This method is applicable to flux classes 1 and 2, as
flux Sample.
defined in ISO 9454-1.
Weigh, to the nearest 0,001 g, approximately 0,5 g
of the solid flux Sample or 2 g of the liquid flux sam-
ple, avoiding loss of volatile matter during the weigh-
3.2 Reagents
ing, and transfer it to a 250 ml low-form beaker.
3.2.1 General
NOTE 3 This procedure is suitable for halide ion concen-
trations generally within the range 0,l % (m/m) to
Only reagents of recognized analytical quality and
1 % (m/m) in the non-volatile content of the Solution to be
distilled or deionized water with a conductivity less
titrated. For flux samples having halide ion concentrations
than 10 pS/cm are to be used.
outside this range, the Sample mass taken should be ad-
justed, as follows:
3.2.2 Propan-2-01.
a) for flux samples having a halide ion concentration in the
3.2.3 Siber nitrate solution (0,02 mol/l). range 0,05 % (m/m) to 0,l % (m/m), the mass of
Sample taken should be double; and
3,4 g of silver nitrate (AgNO,) are dissolved in water
b) for flux samples having a halide ion concentration in the
(see note 1) then transferred to a 1 litre volumetric
range 1 % (m/m) to 2 % (m/m), the mass of Sample
flask and diluted to the mark with water. lt is mixed
taken should be halved.
thoroughly.
Add 100 ml of propan-2-01 (3.2.2), or water, according
Alternatively a commercially available concentrate is
to the solubility characteristics of the flux (see
used to prepare 0,02 mol/1 Standard silver nitrate sol-
note 4). Cover with a watch glass and allow to dis-
ution.
solve with gentle agitation.
The silver nitrate Solution is standardized using the
NOTE 4 For fluxes of class 1.2, as defined in ISO 9454-1
method given in annex A, to derive the correlation
the choice of solvent should be agreed between the flux
factorf,. This is stored in an amber glass bottle.
manufacturer and the User.
NOTES
Place the beaker on the stand of the titration as-
1 The silver nitrate (AgNO,) should be dried at
sembly with the electrodes, stirrer and burette in
110 “C + 5 “C for 16 h and cooled in a desiccator before
-
Position. Adjust the Speed of the stirrer to give vigor-
weighing.
ous stirring without splashing. Titrate with the silver
nitrate Solution (3.2.3), adding 1 ml portions and re-
2 1 ml of silver nitrate Solution (3.2.3) is equivalent to
cording the mV meter readings after each addition.
0,000 709 x.fi g of chloride ion.
As the end-point is approached, reduce the additions
of titrant to 0,l ml and continue titrating past the
end-point.
3.3 Apparatus
Plot the potential values against the volume of titrant
Ordinary laboratory apparatus and
added to obtain the titration curve. The Point of in-
flexion of the curve corresponds to the end-point of
3.3.1 Millivolt meter.
the titration.
3.3.2 Silver electrode.
NOTE 5 The Point of inflexion of the curve may con-
veniently be determined by using the derivative curve.
3.3.3 Mercury/mercurous sulfate 1 mol/1 so-
Carry out a blank determination, using all reagents, for
dium sulfate electrode, or a reversible hydrogen
comparison purposes.
electrode.

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SIST EN ISO 9455-6:2001
Q ISO
ISO 9455-6: 1995(E)
The test is applicable to fluxes of classes 2.1.2.A and
3.5 Calculation of results
3.1 .l .A only, as defined in ISO 9454-1.
The halide (excluding fluoride) content, expressed as
Some liquid fluxes contain free hydrochloric acid and
the percentage, by mass, of chloride in the flux, is
the halide content will, consequently, be greater than
given by:
the amount equivalent to the zinc and other chlorides
0,070 9 x v
present.
f
1
m
4.2 Reagents
V is the volume, in millilitres, of silver nitrate
Solution used, less the volume needed to
4.2.1 General
titrate the blank;
Only reagents of recognized analytical quality and
is the correlation factor for the silver nitrate
f
1
distilled or deionized water with a conductivity less
Solution (see 3.2.3);
than 10 pS/cm are to be used.
m is the mass, in grams, of the Sample taken.
4.2.2 Silver nitrate Solution (0,l mol/l).
The halide content of the flux Sample is given by the
16,99 g of silver nitrate (AgNO,) are dissolved in
mean of the three results obtained on the triplicate
test samples. water (see note 1) then transferred to a 1 litre volu-
metric flask and diluted to the mark with water. This
The halide content may also be expressed as the
is mixed thoroughly.
percentage, by mass, of chloride in the non-volatile
Alternatively, a com mercia Ily available con centrate is
matter by:
used to prepare 0,l mol/1 Standard silver nitrate sol-
7,09 x v
ution.
f 1
mS
The silver nitrate Solution is standardized using the
where
method given in annex A, to derive the correlation
factorf,. This is stored in an amber glass bottle.
is the percentage non-volatile matter con-
S
tent of the Sample, determined as de-
NOTES
scribed in ISO 9455-1 or ISO 9455-2. For
solid flux samples, S = 100. 6 The silver nitrate (AgNO,) should be dried at
110 “C + 5 “C for 16 h and cooled in a desiccator before
-
weighing.
7 1 ml of silver nitrate Solution (4.2.2) is equivalent to
0,003 545 xf2 grams of chloride ion.
4 Method B: Titration method for halide
(excluding fluoride) content of water-
4.2.3 Ammonium thiocyanate Solution (approxi-
soluble fluxes
mately 0,l mol/l).
8 g of ammonium thiocyanate (NHJNS) are dissolved
4.1 Principle
in water then transferred to a 1 litre volumetric flask
and diluted to the mark with water. This is mixed
A prepared Sample of the flux is diluted to a known
thoroughly.
volume with water and a specified volume of sulfuric
acid of known concentration. The Solution is then Alternatively, a commercially available concentrate is
treated with a known quantity of silver nitrate Solution used to prepare 0,l mol/1 Standard ammonium thio-
and the excess silver nitrate is titrated with am- cyanate Solution.
monium thiocyanate. A blank determination using
water in place of the flux is carried out simultaneously 4.2.4 Sulfuric acid Solution [20 % (V/V)]. 200 ml
and the percentage halide content, expressed as of sulfuric acid (density 1,84 g/ml) is cautiously added,
chloride, is calculated. The method is no-t suitable for with stirring, to 400 ml of water. lt is then mixed,
the determination 0% fluoride. cooled, diluted to 1 litre and mixed thoroughly.

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SIST EN ISO 9455-6:2001
0 ISO
ISO 9455-6: 1995(E)
4.25 Ammonium ferric sulfate indicator ammonium ferric sulfate indicator solution (4.2.5) and
solution. titrate with the ammonium thiocyanate Solution
(4.2.3), as in the procedure given in 4.4.
10 g of ammonium ferric sulfate
Calculate the correlation factor f3 for the ammonium
[NH,Fe(S0,)212H,0] are dissolved in 100 ml water.
thiocyanate, as follows:
4.2.6 Nitrobenzene
25 x.h
f3 =
volume of NH,CNS
WARNING - Care should be exercised in the
handling and disposal of this hazardous reagent.
4.6 Calculation of results
4.2.7 Nitrit acid (density 1,42 g/ml).
The halide (excluding fluoride) content, expressed as
the percentage by mass of chloride in the flux, is
4.3 Apparatus
given by the following formula:
(titreblank - titre
x wo3 545 x.h
Ordinary laboratory apparatus. sample)
x 100
0,5 d
1
4.4 Procedure
which simplifies to:
Carry out the following procedure, in triplicate, on the
0,709 x v
f3
flux Sample.
d
By means of a pipette, transfer 25 ml of the Sample
to a 500 ml volumetric flask. Add 10 ml of sulfuric
acid Solution (4.2.4), dilute to the mark with water and
V is the volume, in millilitres, of ammonium
mix. thiocyanate Solution (4.2.3) used in the
titration of the blank, minus the volume
By means of a pipette, transfer 10 ml of this Solution
used in the titration of the flux Sample;
to a glass-stoppered 500 ml conical flask and ad6
50 ml of water, followed by 5 ml of nitric acid (4.2.7).
d is the density, in grams per millilitre, of the
original flux Sample, at 20 “C, determined
To a similar flask transfer 60 ml of water and 5 ml of
by the use of a hydrometer;
nitric acid (4.2.7) and carry out, simultaneously, a
blank determination following the same procedure is the correlation factor for the ammonium
f3
and using the Same quantities of reagents as used for thiocyanate obtained in 4.5.
the flux Sample.
The halide content of the flux Sample is given by the
By means of a burette or a pipette, add 50 ml of silver mean of the three results obtained on the triplicate
nitrate Solution (4.2.2) to the contents of the flask. test samples.
2 ml of nitrobenzene (42.6) may be added to
NOTE 8 NOTE 9 As an alternative practice the original 25 ml
assist coagulation of the precipitate. Sample may be weighed and the final calculation adjusted
accordingly.
Re-stopper the flask and Shake it vigorously. Add
5 ml of ammonium ferric sulfate indicator solution
5 Method C: ‘hitration method for the
(4.2.5) and titrate with ammonium thiocyanate sol-
determination of halide (excluding
ution (4.2.3) shaking the flask vigorously between
additions of the titrant. T
...